Standard Operation Procedure - BR 9200 Spinning Band

Rev 01 Issued By: Kat Lawrence

2020.09.14

Approved By:

Confidential Information

Standard Operation Procedure - BR 9200 Spinning

Band Distillation SOP

Document Number [####]

Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP [Doc

###]Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP


2020.09.15 Approved By: [Approvers Name]

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Table of Contents

Table of Contents .......................................................................................................................................... 1

1. Purpose ................................................................................................................................................ 2

2. Scope .................................................................................................................................................... 2

3. Terminology ......................................................................................................................................... 2

4. Safety .................................................................................................................................................... 2

5. Equipment ............................................................................................................................................ 3

6. Materials .............................................................................................................................................. 3

7. Chain of Custody .................................................................................................................................. 3

8. Record Keeping .................................................................................................................................... 4

9. Equipment Set-Up ................................................................................................................................ 4

10. Procedure ............................................................................................................................................. 6

11. Waste Handling .................................................................................................................................. 10

12. Calculations ........................................................................................................................................ 11

13. References .......................................................................................................................................... 11

14. Appendixes ......................................................................................................................................... 12





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1. Purpose

The purpose of this SOP is to provide instruction for safe loading of the BR9200 Spinning Band

Distillation Unit.

2. Scope

This document is applicable to laboratory operations and employees preforming distillations with

the spinning band unit.

3. Terminology

This section should include abbreviations, definitions, acronyms, key words, or other special terms

contained within the procedure.

Term Definition

SOP Standard Operating Procedure

PPE Personal Protective Equipment

COC Chain of Custody

4. Safety

4.1. Required PPE

• Heat resistant gloves

• Flame Resistant long-sleeved shirts and jeans or pants.

• Latex/Nitrile disposable gloves

• Closed-toe shoes that are chemical resistant and have non-skid soles

• Safety glasses with side shields

• Goggles (where there is a potential for splashing liquids)

• Long hair should be tied back and tucked under lab coat.





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• Hanging/dangling jewelry should be tucked into clothing or removed prior to working with

equipment).

4.2. Other PPE may be required in addition to, or in place of, the above list.

4.3. General Safety Information

• Before following this SOP, you must review the user manual for the BR9200.

• Do not operate this equipment if you have not been trained to do so.

• Do not apply pressure to this system, it is designed to be used under a vacuum.

• Do not operate this equipment if it is in less than perfect condition.

• Do not plug or unplug anything unless all switches are in the off position.

4.4. HSE Risks

• Hot surfaces can cause scalding/burns. Always allow equipment and glassware to cool prior

to handling.

• Glass components can break, broken glass can cut/puncture the skin. Handle with caution

to avoid breakages.

• Malfunctions or hazardous operating conditions that may affect personnel safety require

shut down and disconnection from power. Equipment will require proper restoration to the

normal operational state before the equipment can be used.

5. Equipment

5.1. Required Equipment

• BR9200 Spinning Band Distillation Unit

• Heating Mantle (1L, 5L, and 22L depending on Batch Size)

• Boiling Flasks (1L, 5L, and 22L depending on Batch Size)

• 1 L Receiving Flasks

• 4 L Receiving Flasks

• Distillation Notebook

6. Materials

6.1. The following materials are examples of acceptable feeds for this SOP

6.1.1. Winterized, decarboxylated Extract

6.1.2. Extract that has passed through a 5um filter at -60C.

7. Chain of Custody

To be addressed according to state guidelines utilizing Metrc and Lab Databases.





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8. Record Keeping

8.1. Records are to be kept in the ‘Distillations’ Notebook and Lab Database:

8.1.1. Date

8.1.2. Feed Extract Metrc Tag Numbers and Quantities

8.1.3. Distillate Metrc Tag Number and Quantities

8.1.4. Terpene Fraction weights.

8.1.5. Pot Bottom Metrc Tag Numbers and Quantities

8.1.6. Product Batch ID (See Appendix B for instructions on Batch ID generation)

8.1.7. Production Batch Metrc Tag Number

8.2. Additional data is logged by the PC including temperatures, vacuum levels, and set points.

9. Equipment Set-Up

9.1. Please refer to BR9200 Manual for equipment set-up information.

9.2. The BR9200





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9.3. The Cold Trap





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9.4. The Fraction Collector

10. Procedure

10.1. Please refer to BR9200 Manual for operational procedure.

10.2. Turning on the system

10.2.1. Turn on the power to the controller. The switch is located on the front panel of the

microprocessor. 1 is for on and 0 is for off.

10.2.2. When power is applied, the controller will sound a brief audible alarm test. The

following screen will be displayed:

B/R Instrument M690

Please Wait

Running System Test

10.2.3. Once the system test is successfully completed, the following screen will be displayed.

B/R Instrument M690

Select a Command Key

10.2.4. Turn on the PC and open the B/R Icon on the desktop. The small keypad of the M690

will now read:

USB Operation

Keypad Disabled





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10.2.5. From the PC Desktop select the B/R Icon. From Manual Controls a vacuum test can be

performed, and the condenser bath can be turned on and pre-cooled.

10.3. Pre-Cooling the Distillation System and Vacuum Check

10.3.1. Make sure the distillation system is clean and dry.

10.3.2. Assemble the distillation system and perform a full vacuum test and achieve a vacuum

below 0.1 mmHg. If the distillation system does not pass the vacuum test, use the

procedure for finding a vacuum leak before proceeding.

10.3.3. Cool the cold trap for a minimum of 2 hours. Longer is better. If possible, leave the cold

finger on overnight.

10.3.4. Start the condenser bath in manual controls and make the set point -20 °C. Let it cool till

it reaches at least -10 °C.

10.4. Preparing the Distillation System

10.4.1. After ethanol recovery and decarboxylation, the warm extract shall be transferred into

an appropriately sized boiling flask for distillation. Flasks should never be filled past 80% of

their capacity, the following Table indicates appropriate sizing information for boiling pot

selection.

Boiling Flask

Size

Minimum Quantity of

Extract Required

Maximum Quantity

of Extract Allowed

1 liter 500 grams 800 grams



10.4.2. The heating mantle appropriate to the flask selected for the distillation should be placed

in the distillation unit and plugged into the control board.

10.4.2.1. The boiling flask containing decarboxylated distillate should be placed into the

mantle, and the platform should be raised to ensure a proper seal between the

boiling flask and the column.

10.4.2.2. Warning!!! Do not leave any residue on the exterior of the boiling flask. Do not

spill anything on the heating mantle. These can cause heating mantle failure.

10.4.2.3. Warning!! Do not overtighten the lab jack as this may damage the distillation

column.

10.4.2.4. Verify that the receivers in the fraction collector are in place and are empty.

10.4.2.5. Verify that the fraction collector is assembled and connected to the distillation

system.





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10.4.2.6. Verify Cold Fingers are in place and empty.

10.4.2.7. Make sure you have the thermowell and temperature probe in the boiling flask.

Apply vacuum grease to the boiling flask thermowell. Check the temperature probe

in the head for proper placement. Close door for safety.

10.4.2.8. If you are going to perform an atmospheric distillation, Open the Vent Valve.

10.4.2.9. If you are going to perform a vacuum distillation, Close the Vent Valve.

10.4.2.10. Correct Valve Positions for starting a Distillation:

10.4.2.10.1. Valve #1 in pointing upward means you have sealed off Distillation head

to allow full vac.

10.4.2.10.2. Valve #2 pointing to the left allows vac on collection vessel.

10.4.2.10.3. Valve #3 in the upright position means system is fully open to vac

10.4.2.10.4. Valve #3 in the closed position means you have isolated the collection

flask.

10.4.2.10.5. See BR Manual for troubleshooting and vacuum testing.

10.5. Performing a Distillation.

10.5.1. From the PC Desktop press the BR ICON. The main menu screen will appear on the PC.

10.5.2. Select the Start Distillation button and the library of distillation runs will appear.

10.5.3. Select the distillation run which corresponds to the material you are distilling. A series of

questions/reminders will be displayed. After acknowledging the questions, the Process

Run screen will appear. There are several options.

10.5.3.1. The Run Data Screen allows the distillation parameters to be viewed and edited.

10.5.3.2. The Run Tuning Screen allows certain “Hot Keys” to be accessed. The spinning

band motor, reflux valve, fraction collector and some other functions can have their

functions briefly tested.





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10.5.3.3. The Process Diagram allows the current state of the distillation to be viewed

along with the schematic of the distillation equipment. The actual schematic

displayed will depend on the configuration selected in System Options.

10.5.3.4. The Run Data Screen is the most common screen to use to operate the

distillation. The distillation can be paused at any time by selecting the Pause button.

Once paused, the distillation can be Aborted or Resumed.

10.5.3.5. You can edit any parameter during the distillation run in the Run Data screen.

Once you enter a new parameter you will need to press ENTER to confirm your

parameter change.

10.5.3.6. At the bottom of each screen is a bar which displays the real time parameters

of the distillation. Vapor, Pot and Condenser Temperatures, vacuum level and

heating rate are displayed.

10.5.3.7. Distillation begins at 50 mmHg vacuum set point.

10.5.3.8. As boiling flask heats up, you’re able to slowly reduce vacuum.

10.5.3.8.1. Caution- Only reduce vacuum in 10 unit increments or less.

10.5.3.9. Residual ethanol will come off first then Terpenes.

10.5.3.9.1. Properly winterized material will have minimal ethanol, we may see up

to 200mL ethanol collected in a large distillation of 19L of feed.

10.5.3.10. Only lower vacuum set points as Distillation slows down to speed up the run. Be

careful not to push the limits.

10.5.3.11. At approximately 30 mmHg and 105c boiling flask temperature the

decarboxylation begins. CO2 will emit from the sample and the vacuum will not be

able to be reduced further until Decarboxylation is completed.

10.5.3.11.1. If feed material was previously decarboxylated, there will be no

vacuum/ temperature plateau and the run will continue to the next step.

10.5.3.12. Typically, residual ethanol will continue until you reach 160-170c. at this point

terpenes will roll off until oil starts to run.

10.5.3.13. Set points on chiller start at -20C through residual ethanol distillation.

10.5.3.14. As terpenes roll off the chiller temp should be increased to -10C briefly before

increasing the temperature to 0C.

10.5.3.15. As terpenes begin to slow down its time to raise chiller temperature 20c.





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10.5.3.16. When boiling flask reaches 190C vac set points should be as low as possible;

0.01 mmHg. Chiller should be set to 55C.

10.5.3.17. Look for smoke rings with a controlled light pops in boiling flask. This means

THC9 is ready to come out. Always remember that either green oil or azuline comes

off fist followed by main body.

10.5.3.18. When collecting oil make sure to collect main body with no tails.

10.6. Finishing a Distillation

10.6.1. When the distillation is complete, you can hit pause and then abort of the run.

10.6.2. Turn off the vacuum pump, and chillers. This will stop heating the unit; however it will

remain under vacuum until you open the vent.

10.6.3. You can isolate your fraction collector and receivers from the remainder of the system

by closing valve 3.

10.6.4. Then open valve 2 slowly to equalize the pressure in the fraction collector.

10.6.5. You are now able to open the fraction collector to remove the distillate product while

leaving the bulk of the system under vacuum to cool.

10.6.5.1. The distillate in the receivers is now ethanol free delta 9 THC distillate, it is no

longer considered hazardous. Weights and volumes should be recorded. The

distillate can be warmed and transferred to a large beaker for homogenization and

testing.

10.6.6. Once the distillation unit is cool, open valve 1 to eliminate the vacuum.

10.6.7. At this point you can remove the boiling pot flask and determine the mass of material

still in the flask. This is the heavies from the distillation, and the heavies will be combined

with other distillation heavies for future re-distillation.

11. Waste Handling

All solvents shall be recycled internally; undergo purification via additional rotary evaporator distillation

or by distillation in the spinning band unit, once purity can be confirmed the purified solvent can be

used again. Solvent waste shall be handled according to state and federal guidelines, following the Lab

Waste Handling SOP.





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12. Calculations

12.1.

13. References

13.1.1. Operating Manual Model 9200 Fractional Spinning Band Distillation System; BR

Instrument Corporation





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14. Appendixes

14.1. Appendix A. Production Batch ID:

14.1.1. The production batch ID will consist of the strain abbreviation (if more than one list all

separated by periods), followed by an underscore, then either Terp1, Terp2, Terp#,

THC9Dist1, THC9Dist2, etc for the distillate cut or Heavies for the pot bottoms , then the

date YYYY.MM.DD, followed by an underscore, then the last 4 digits of the New Metrc

batch tag ID. Cold Fingers will be labeled CFLT, CFMT, CFHT in the same mannor.

14.1.1.1. Example 1: You are labelling your main body of distillate for the day, and the

New Batch Metrc tag will end in 2127. The date is 2020.08.15, this distillate was from

99 Problems, the Batch ID would look like this:

99D1_THC9Dist1.2020.08.15_2127

14.1.1.2. Example 2: You are labelling your pot bottoms (heavies) August 15th, 2020. The

feed was 99 Problems extract and the batch Metrc tag will end in 2128. The Batch ID

would look like this:

99D1_Heavies.2020.08.15_2128





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14.2. Appendix B. Cloud Cover Strain Abbreviations

Strain Abbreviation

99 Problems #1 99D1

Alien Pie AP

Cherry Punch CP

Coogies CG

Do-Si-Dos DSD

Flo FLO

Frozen Dessert FD

Ghost Dawg GD

GMO GMO

Gorilla Glue #4 GG4

Grape Stomper GS

Headbanger HB

GSC GSC

Headbanger HB

Ice Cream Cke ICC

Katsu Bubba Kush BK

Lemon Ozium LO

Lemon Ozium #1 LO1

Mentoz MTZ

Orange Ghost OJG

Power Nap PN

Presidential Kush PREZ

Queso Perro QP

Sour Tangie ST

Triangle Kush TK

UK Cheese UK

White 99 W99

Wookie Girl '91 WG

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Standard Operation Procedure - BR 9200 Spinning Band